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#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051881.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7051881
loop_
_publ_author_name
'Burchell, Tara J.'
'Enright, Gary D.'
'Ripmeester, John A.'
_publ_section_title
;
 Guest capture, storage and removal in the TATM host framework: a
 single-crystal study
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              864
_journal_paper_doi               10.1039/b718592h
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         '2(C19H16O3S3) 0.21(C2H4Cl2)'
_chemical_formula_sum            'C38.42 H32.84 Cl0.42 O6 S6'
_chemical_formula_weight         797.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.368(6)
_cell_angle_beta                 106.028(6)
_cell_angle_gamma                95.933(6)
_cell_formula_units_Z            1
_cell_length_a                   7.964(4)
_cell_length_b                   10.792(5)
_cell_length_c                   12.002(6)
_cell_measurement_reflns_used    7143
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.69
_cell_volume                     975.6(8)
_computing_cell_refinement       'SAINT (Bruker 2001)'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10240
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.8834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             415
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3934
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0634P)²+5.4700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2144
_refine_ls_wR_factor_ref         0.2275
_reflns_number_gt                3092
_reflns_number_total             3934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718592h.txt
_cod_data_source_block           2d
_cod_database_code               7051881
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.6456(5) -0.0667(4) 0.1479(4) 0.0290(9) Uani 1 1 d U . .
O2 O 0.0601(6) 0.4643(4) -0.2431(4) 0.0325(10) Uani 1 1 d U . .
O3 O 0.4681(6) 0.4268(4) 0.6716(4) 0.0424(11) Uani 1 1 d U . .
S1 S -0.42138(17) 0.17047(13) 0.15613(13) 0.0240(4) Uani 1 1 d U . .
S2 S 0.24744(17) 0.45841(12) 0.00871(13) 0.0227(3) Uani 1 1 d U . .
S3 S 0.4103(2) 0.19770(16) 0.50041(14) 0.0339(4) Uani 1 1 d U . .
C1 C 0.0937(6) 0.1756(5) 0.1706(4) 0.0164(10) Uani 1 1 d U . .
H1 H 0.1311 0.0959 0.1406 0.020 Uiso 1 1 calc R . .
C2 C -0.1025(6) 0.1465(5) 0.1616(4) 0.0184(10) Uani 1 1 d U . .
C3 C -0.1879(6) 0.0232(5) 0.1571(4) 0.0186(10) Uani 1 1 d U . .
H3 H -0.1314 -0.0501 0.1557 0.022 Uiso 1 1 calc R . .
C4 C -0.3618(7) 0.0216(5) 0.1550(5) 0.0193(11) Uani 1 1 d U . .
C5 C -0.2133(7) 0.2339(5) 0.1614(5) 0.0197(11) Uani 1 1 d U . .
H5 H -0.1788 0.3213 0.1639 0.024 Uiso 1 1 calc R . .
C6 C -0.4952(7) -0.0847(5) 0.1493(5) 0.0217(11) Uani 1 1 d U . .
C7 C -0.4404(8) -0.2136(6) 0.1504(6) 0.0332(14) Uani 1 1 d U . .
H7A H -0.5457 -0.2773 0.1261 0.050 Uiso 1 1 calc R . .
H7B H -0.3703 -0.2216 0.2298 0.050 Uiso 1 1 calc R . .
H7C H -0.3695 -0.2263 0.0962 0.050 Uiso 1 1 calc R . .
C8 C 0.1227(6) 0.2730(5) 0.0919(5) 0.0175(10) Uani 1 1 d U . .
C9 C 0.0219(6) 0.2611(5) -0.0267(5) 0.0194(11) Uani 1 1 d U . .
H9 H -0.0724 0.1950 -0.0630 0.023 Uiso 1 1 calc R . .
C10 C 0.0733(6) 0.3544(5) -0.0844(5) 0.0190(11) Uani 1 1 d U . .
C11 C 0.2493(7) 0.3766(5) 0.1221(5) 0.0208(11) Uani 1 1 d U . .
H11 H 0.3295 0.4003 0.1984 0.025 Uiso 1 1 calc R . .
C12 C 0.0027(7) 0.3737(5) -0.2061(5) 0.0258(12) Uani 1 1 d U . .
C13 C -0.1444(10) 0.2797(7) -0.2854(6) 0.0477(18) Uani 1 1 d U . .
H13A H -0.2576 0.3079 -0.2858 0.071 Uiso 1 1 calc R . .
H13B H -0.1391 0.1979 -0.2574 0.071 Uiso 1 1 calc R . .
H13C H -0.1330 0.2717 -0.3650 0.071 Uiso 1 1 calc R . .
C14 C 0.2008(6) 0.2119(5) 0.2979(5) 0.0202(11) Uani 1 1 d U . .
C15 C 0.2013(7) 0.3240(5) 0.3707(5) 0.0225(11) Uani 1 1 d U . .
H15 H 0.1335 0.3883 0.3447 0.027 Uiso 1 1 calc R . .
C16 C 0.3094(7) 0.3309(5) 0.4827(5) 0.0243(12) Uani 1 1 d U . .
C17 C 0.3089(7) 0.1344(5) 0.3573(5) 0.0266(12) Uani 1 1 d U . .
H17 H 0.3255 0.0548 0.3228 0.032 Uiso 1 1 calc R . .
C18 C 0.3560(8) 0.4353(6) 0.5804(5) 0.0278(13) Uani 1 1 d U . .
C19 C 0.2660(8) 0.5489(6) 0.5659(5) 0.0326(14) Uani 1 1 d U . .
H19A H 0.3490 0.6239 0.6079 0.049 Uiso 1 1 calc R . .
H19B H 0.1653 0.5412 0.5978 0.049 Uiso 1 1 calc R . .
H19C H 0.2244 0.5566 0.4825 0.049 Uiso 1 1 calc R . .
Cl1 Cl 0.780(3) 0.0947(19) 0.4463(16) 0.033(5) Uiso 0.10 1 d PD A 1
C20 C 0.940(4) -0.006(4) 0.4396(13) 0.019(10) Uiso 0.10 1 d PD . 1
H20A H 0.8830 -0.0939 0.4115 0.023 Uiso 0.10 1 calc PR . 1
H20B H 1.0066 0.0201 0.3855 0.023 Uiso 0.10 1 calc PR . 1
Cl2 Cl 0.808(2) 0.1256(18) 0.4438(15) 0.030(5) Uiso 0.11 1 d PD B 2
C21 C 0.982(8) 0.058(5) 0.531(3) 0.06(2) Uiso 0.11 1 d PD . 2
H21A H 1.0902 0.1207 0.5560 0.071 Uiso 0.11 1 calc PR . 2
H21B H 0.9520 0.0384 0.6025 0.071 Uiso 0.11 1 calc PR . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 S1 C4 91.2(2) . . ?
C11 S2 C10 91.8(3) . . ?
C17 S3 C16 91.5(3) . . ?
C14 C1 C8 114.2(4) . . ?
C14 C1 C2 109.8(4) . . ?
C8 C1 C2 110.8(4) . . ?
C5 C2 C3 111.9(5) . . ?
C5 C2 C1 124.9(5) . . ?
C3 C2 C1 123.1(4) . . ?
C4 C3 C2 112.4(5) . . ?
C3 C4 C6 129.8(5) . . ?
C3 C4 S1 111.4(4) . . ?
C6 C4 S1 118.7(4) . . ?
C2 C5 S1 113.0(4) . . ?
O1 C6 C4 120.1(5) . . ?
O1 C6 C7 121.8(5) . . ?
C4 C6 C7 118.1(5) . . ?
C11 C8 C9 111.4(5) . . ?
C11 C8 C1 126.4(5) . . ?
C9 C8 C1 122.1(4) . . ?
C10 C9 C8 113.5(5) . . ?
C9 C10 C12 129.6(5) . . ?
C9 C10 S2 110.5(4) . . ?
C12 C10 S2 119.9(4) . . ?
C8 C11 S2 112.8(4) . . ?
O2 C12 C10 121.5(5) . . ?
O2 C12 C13 120.0(6) . . ?
C10 C12 C13 118.5(5) . . ?
C17 C14 C15 111.7(5) . . ?
C17 C14 C1 122.3(5) . . ?
C15 C14 C1 126.0(5) . . ?
C16 C15 C14 113.3(5) . . ?
C15 C16 C18 129.5(5) . . ?
C15 C16 S3 111.2(4) . . ?
C18 C16 S3 119.1(4) . . ?
C14 C17 S3 112.4(4) . . ?
O3 C18 C16 119.4(6) . . ?
O3 C18 C19 121.6(5) . . ?
C16 C18 C19 119.0(5) . . ?
C20 C20 Cl1 106.4(19) 2_756 . ?
C21 C21 Cl2 113(2) 2_756 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C6 1.229(6) . ?
O2 C12 1.217(7) . ?
O3 C18 1.226(7) . ?
S1 C5 1.708(5) . ?
S1 C4 1.721(5) . ?
S2 C11 1.700(6) . ?
S2 C10 1.726(5) . ?
S3 C17 1.711(6) . ?
S3 C16 1.723(6) . ?
C1 C14 1.515(7) . ?
C1 C8 1.530(7) . ?
C1 C2 1.533(7) . ?
C2 C5 1.356(7) . ?
C2 C3 1.419(7) . ?
C3 C4 1.376(7) . ?
C4 C6 1.463(7) . ?
C6 C7 1.501(8) . ?
C8 C11 1.369(7) . ?
C8 C9 1.412(7) . ?
C9 C10 1.373(7) . ?
C10 C12 1.459(8) . ?
C12 C13 1.494(9) . ?
C14 C17 1.375(8) . ?
C14 C15 1.410(8) . ?
C15 C16 1.371(8) . ?
C16 C18 1.470(8) . ?
C18 C19 1.486(9) . ?
Cl1 C20 1.770(10) . ?
C20 C20 1.48(2) 2_756 ?
Cl2 C21 1.769(10) . ?
C21 C21 1.49(2) 2_756 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C5 83.5(6) . . . . ?
C8 C1 C2 C5 -43.5(7) . . . . ?
C14 C1 C2 C3 -93.8(6) . . . . ?
C8 C1 C2 C3 139.1(5) . . . . ?
C5 C2 C3 C4 -0.7(7) . . . . ?
C1 C2 C3 C4 177.0(5) . . . . ?
C2 C3 C4 C6 179.3(5) . . . . ?
C2 C3 C4 S1 1.0(6) . . . . ?
C5 S1 C4 C3 -0.8(4) . . . . ?
C5 S1 C4 C6 -179.3(4) . . . . ?
C3 C2 C5 S1 0.1(6) . . . . ?
C1 C2 C5 S1 -177.5(4) . . . . ?
C4 S1 C5 C2 0.3(4) . . . . ?
C3 C4 C6 O1 -179.8(5) . . . . ?
S1 C4 C6 O1 -1.6(7) . . . . ?
C3 C4 C6 C7 2.8(9) . . . . ?
S1 C4 C6 C7 -179.0(4) . . . . ?
C14 C1 C8 C11 9.4(7) . . . . ?
C2 C1 C8 C11 134.0(5) . . . . ?
C14 C1 C8 C9 -173.7(4) . . . . ?
C2 C1 C8 C9 -49.1(6) . . . . ?
C11 C8 C9 C10 0.4(6) . . . . ?
C1 C8 C9 C10 -176.9(4) . . . . ?
C8 C9 C10 C12 179.7(5) . . . . ?
C8 C9 C10 S2 -0.3(6) . . . . ?
C11 S2 C10 C9 0.1(4) . . . . ?
C11 S2 C10 C12 -179.9(4) . . . . ?
C9 C8 C11 S2 -0.3(6) . . . . ?
C1 C8 C11 S2 176.8(4) . . . . ?
C10 S2 C11 C8 0.1(4) . . . . ?
C9 C10 C12 O2 177.6(5) . . . . ?
S2 C10 C12 O2 -2.4(7) . . . . ?
C9 C10 C12 C13 -1.8(9) . . . . ?
S2 C10 C12 C13 178.2(5) . . . . ?
C8 C1 C14 C17 -126.2(5) . . . . ?
C2 C1 C14 C17 108.7(6) . . . . ?
C8 C1 C14 C15 55.3(7) . . . . ?
C2 C1 C14 C15 -69.8(6) . . . . ?
C17 C14 C15 C16 0.5(7) . . . . ?
C1 C14 C15 C16 179.2(5) . . . . ?
C14 C15 C16 C18 174.6(5) . . . . ?
C14 C15 C16 S3 -0.8(6) . . . . ?
C17 S3 C16 C15 0.6(4) . . . . ?
C17 S3 C16 C18 -175.3(4) . . . . ?
C15 C14 C17 S3 0.0(6) . . . . ?
C1 C14 C17 S3 -178.8(4) . . . . ?
C16 S3 C17 C14 -0.3(4) . . . . ?
C15 C16 C18 O3 -173.6(6) . . . . ?
S3 C16 C18 O3 1.5(7) . . . . ?
C15 C16 C18 C19 6.2(9) . . . . ?
S3 C16 C18 C19 -178.7(4) . . . . ?
H1 C1 C2 C5 -160.2 . . . . ?
H1 C1 C8 C11 -109.2 . . . . ?
H1 C1 C14 C17 -7.5 . . . . ?
